US5045437A - Method for producing a structured ceramic film or a ceramic member constructed of such films by sintering and useful as ultrasound transducers - Google Patents

Method for producing a structured ceramic film or a ceramic member constructed of such films by sintering and useful as ultrasound transducers Download PDF

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Publication number
US5045437A
US5045437A US07/432,724 US43272489A US5045437A US 5045437 A US5045437 A US 5045437A US 43272489 A US43272489 A US 43272489A US 5045437 A US5045437 A US 5045437A
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Prior art keywords
green
film
films
photoresist layer
ceramic
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Expired - Lifetime
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US07/432,724
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English (en)
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Ulrich Bast
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Siemens AG
Eastman Kodak Co
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Siemens AG
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Assigned to SIEMENS AKTIENGESELLSCHAFT reassignment SIEMENS AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: BAST, ULRICH
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Assigned to INKJET SYSTEMS GMBH & CO. KG reassignment INKJET SYSTEMS GMBH & CO. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: EASTMAN KODAK COMPANY
Assigned to EASTMAN KODAK COMPANY reassignment EASTMAN KODAK COMPANY CORRECTION OF RECORDATION OF ASSIGNMENT RECORDED AT REEL 7201, FRAMES 578-605 Assignors: INKJET SYSTEMS GMBH 7 CO.KG
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/002—Producing shaped prefabricated articles from the material assembled from preformed elements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/008—Bodies obtained by assembling separate elements having such a configuration that the final product is porous or by spirally winding one or more corrugated sheets
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/30—Stacked capacitors
    • H01G4/304—Stacked capacitors obtained from a another capacitor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
    • H01L21/4803—Insulating or insulated parts, e.g. mountings, containers, diamond heatsinks
    • H01L21/4807—Ceramic parts
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/08—Shaping or machining of piezoelectric or electrostrictive bodies
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/093—Forming inorganic materials
    • H10N30/097—Forming inorganic materials by sintering
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H05K1/0306—Inorganic insulating substrates, e.g. ceramic, glass
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/0011—Working of insulating substrates or insulating layers
    • H05K3/0044—Mechanical working of the substrate, e.g. drilling or punching

Definitions

  • the present invention is directed to a method for producing a structured ceramic film. Further, the invention is directed to the manufacture of a ceramic member composed of such ceramic films.
  • the structuring of such a ceramic film is comprised in depressions or, respectively, recesses that can also be holes that proceed through the film.
  • the production of the depressions, recesses or holes thereby ensues by processing the film in the condition of a green film.
  • a green film is the intermediate stage occurring in the manufacturing method of a ceramic film wherein the suspension material to be subsequently sintered to form a ceramic and having the bonding agent or, respectively, binding system contained therein is brought into the shape of the as yet unsintered film.
  • a known method of this species is to provide the green film composed of the suspension material and the binder system and acquired by drawing the suspension into a film with holes by punching and, finally, to sinter this structured green film.
  • a thin ceramic film provided with these holes that corresponds to the thickness of the green film is thereby obtained, this ceramic film being capable of being employed, for example, as a substrate plate.
  • Such substrate plates particularly those of aluminum oxide, are especially employed in electronic circuit technology for formatting hybrid circuits.
  • German published application 14 39 702 discloses a manufacturing method wherein cavities are already present in the ceramic member before the sintering of the ceramic member provided for a capacitor.
  • the ceramic members coming into consideration here were manufactured in such fashion that individual green films were first provided with a structured photoresist layer or, respectively, with structures composed of photoresist in a photolithographic way and these films were then pressed to form a stack and were sintered.
  • the stack that is sintered together forms a monolithic ceramic member in whose interior cavities that correspond to the photolithographic structures on the original green films are situated.
  • the photoresist burns off during the sintering process and leaves corresponding cavities in the foil stack.
  • Such cavities can be arranged exactly placed in a ceramic member (and, for example, can serve as electrodes when filled with metal).
  • An object of the present invention is to specify a method that is especially simple in technological terms with whose assistance such ceramic films (as yet unsintered) structured with depressions, recesses or holes can be manufactured.
  • a development of the object is comprised in exploiting this method such that ceramic members provided with defined cavities an be manufactured with a method for producing a ceramic film having depressions, holes, recesses and the like, whereby the structuring of the film ensues in the condition thereof as green film having a binder system contained therein, ensuing with the assistance of photolithography which is characterized by a surface of the green film being provided with a photoresist layer and which structures having a prescribed planer distribution and size of the depressions, holes, recesses and the like to be produced are produced in a photolithographic way for employment as a mask, in that the depressions, holes, recesses and the like are produced down to a respectively prescribed depth in the green film by erosion with a liquid jet, whereby the structured photoresist layer is effective as a mask.
  • the present invention also provides a method for producing sintered members having inwardly disposed cavities in which a plurality of green films are produced with depressions, holes, recesses or the like according to the foregoing described method steps are then stacked on top of one another, pressed and subsequently sintered.
  • green films which are produced according to the foregoing may also be stacked with non-structured green films, pressed and subsequently sintered.
  • the monolithic member of piezo ceramic manufactured according to the foregoing steps may be used for ultrasound transducers.
  • the term "ceramic film” is understood to include “ceramic tape”. The production of ceramic tape is by a process known as tape casting.
  • photoresist layer or dry resist layer/film (referred to as photoresist below) composed, for example, of the material Kalle, Ozatec R225 is applied onto the one surface of a green film (still unsintered) produced according to standard method.
  • this photo-sensitive layer is structured into a mask layer that has holes, recesses or the like extending down to the surface of the green film at those locations at which the green film and the ceramic film manufactured later should exhibit holes or, respectively, cavities.
  • this green film is charged with a thin liquid jet on that side provided with the photoresist, an erosion that leads to the production of the depressions that are then present later being carried out with this liquid jet.
  • a typical diameter of such a jet amounts to 0.6 mm.
  • the solvent provided for the jet i.e. the solvent contained therein, is such a solvent that acts to the effect of bringing the binder system or, respectively, a constituent of the binder system to initial swelling such that the following, erosive removal of material of the green film is enabled. This erosive removal is carried out with high jet pressure.
  • Work can also be carried out with a comparatively large-area jet or can be simultaneously carried out with a plurality of or, respectively, with many jets.
  • the solvent is selected such that the binder of the ceramic foil but not the photoresist material itself is attacked.
  • the afore-mentioned photoresist material Ozatec R225 and a binder system provided for the green film on the basis of acrylic acid ester is an advantageous combination with which toluol or a mixture of toluol and decahydronaphthaline can be very advantageously employed, for example in a ratio of 3:2.
  • a material given which higher chemical resistance can be additionally effected by re-exposure or by tempering at high temperature is particularly employed as photoresist.
  • An additional metal film that allows higher resistance to be achieved can also be employed.
  • the photoresist that is still present on the green film is dissolved.
  • positive photoresist for example, an exposure and developing of the photoresist that is now surface-wide is suitable.
  • the photoresist material that is still present is thus rendered soluble and can be easily removed.
  • green films provided with depressions or, respectively, holes in accord with the above method steps are stacked and are exposed to a pressing power at elevated temperature.
  • the foil stack composed of the original green films is sintered to form a monolithic ceramic block that, however, contains the previously produced depressions and holes of the individual green films as cavities.
  • Such a monolithic ceramic member comprising cavities produced according to the method and distributed in a prescribed fashion is subjected to further processing steps; for example, metallization for producing electrodes, the required polarizing with which the piezoelectric properties become effective are carried out.
  • materials processing with a liquid jet is known per se.
  • steel plates are cut with a water jet.
  • a process that is two-stage in principle is carried out, namely, by selecting the composition of the liquid with reference to the material to be processed, namely the binder thereof, one effect is that a swelling and, thus, a corresponding reduction in the strength of the material of the green film occurs.
  • the material treated in this fashion that has thus been lent a property different from the original material of the green film is then separated and rinsed away by the liquid jet treatment.
  • the inventively employed processing method produces no heating in the processed material. Over and above this, by contrast, the liquid jet is even capable of cooling. Large surfaces can be structured in a short time; in particular, they can be eroded surface-wide. The afore-mentioned absence of heating makes any and all warping of the desired shapes impossible.
  • the organic binder is not gaseously decomposed given employment of the invention but is washed out in liquid form. This prevents deposits otherwise appearing due to condensation of the decomposition products at cooler parts (of the apparatus) from being present. Loosened material is removed by the washing and can be easily separated. Dusts cannot occur, so that appropriate work rules can also be managed in a simple way.
  • the measures employed in the invention are suitable precisely for the erosion of great quantities, they are also advantageous for superfine structures.
  • the depth of the structuring can be easily reliably set with these measures (for example, more easily than with laser emission).
  • German Published Application 21 42 535 recites that lead oxides and titanium oxides can be easily converted into metallic lead and titanium with the processing laser emission. Given the temperatures that occur, part of this lead is present in vapor form.
  • FIG. 1 shows a monolithic, sintered ceramic member 1 manufactured according to the invention that comprises channel-like cavities referenced 2 that are designed and positioned in terms of execution and position as may be seen from FIG. 1.
  • such a monolithic ceramic member 1 is manufactured in such fashion that a multitude of green films are produced, as the example of FIG. 2 shows.
  • the green films can be composed of compositions for sintered piezo ceramic, substrate ceramic and the like, for example of lead zirconate titanate, aluminum oxide, etc.
  • the green film 11 in FIG. 2 has already been coated surface-wide with a layer 12 of photoresist material.
  • This photoresist layer 12 is provided with the structure 112 shown in FIG. 3 in a standard photolithographic way. In individual strips 13, the material of the photoresist layer 12 has been eliminated to such an extent that the original surface 14 of the green film 11 is exposed.
  • the structures 112 have dimensions down to, for example, 50 ⁇ m in accord with the essentially identically sized dimensions of the depressions, cavities, holes and the like to be produced in the green film or, respectively, in the finished member.
  • FIG. 4 shows the charging of the green film 11 with a liquid jet 21, namely as seen proceeding from the side provided with the photoresist layer 12.
  • FIG. 5 shows two green films 111 that have been processed in accord with the method of the invention and shows two unmodified green films 11.
  • such films 111, 11, 111, 11 . . . are stacked on top of one another in the way that proceeds from this figure.
  • Such a compressed stack is sintered in a way that is standard per se, so that a monolithic ceramic member 1 having the channels 2 contained therein arises therefrom

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Devices For Post-Treatments, Processing, Supply, Discharge, And Other Processes (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Particle Formation And Scattering Control In Inkjet Printers (AREA)
  • Micromachines (AREA)
  • Ceramic Capacitors (AREA)
  • Laminated Bodies (AREA)
US07/432,724 1987-04-27 1988-04-27 Method for producing a structured ceramic film or a ceramic member constructed of such films by sintering and useful as ultrasound transducers Expired - Lifetime US5045437A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3713987 1987-04-27
DE19873713987 DE3713987A1 (de) 1987-04-27 1987-04-27 Verfahren zur herstellung einer strukturierten keramikfolie bzw. eines aus solchen folien aufgebauten keramikkoerpers

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US5045437A true US5045437A (en) 1991-09-03

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US07/432,724 Expired - Lifetime US5045437A (en) 1987-04-27 1988-04-27 Method for producing a structured ceramic film or a ceramic member constructed of such films by sintering and useful as ultrasound transducers

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US (1) US5045437A (de)
EP (1) EP0362213B1 (de)
JP (1) JPH02500427A (de)
DE (2) DE3713987A1 (de)
WO (1) WO1988008360A1 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1174766A2 (de) * 2000-07-12 2002-01-23 E.I. Du Pont De Nemours And Company Verfahren zur Strukturierung einer nicht-bilderzeugenden keramischen Schicht
US20130022809A1 (en) * 2011-07-18 2013-01-24 Technische Universitaet Wien Multilayer Ceramic Structure and Method for Producing the Same

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US4896464A (en) * 1988-06-15 1990-01-30 International Business Machines Corporation Formation of metallic interconnects by grit blasting
US5170245A (en) * 1988-06-15 1992-12-08 International Business Machines Corp. Semiconductor device having metallic interconnects formed by grit blasting
DE3835794A1 (de) * 1988-10-20 1990-04-26 Siemens Ag Verfahren zur herstellung einer strukturierten keramikfolie bzw. eines aus solchen folien aufgebauten keramikkoerpers
DE4019380C1 (de) * 1990-06-18 1991-12-05 Du Pont De Nemours (Deutschland) Gmbh, 6380 Bad Homburg, De
FR2665699A1 (fr) * 1990-08-07 1992-02-14 Thomson Csf Ceramique piezoelectrique a porosite controlee.
JP2861368B2 (ja) * 1990-11-05 1999-02-24 住友電気工業株式会社 回路基板の加工方法
WO1994002294A1 (de) * 1992-07-15 1994-02-03 Hoechst Ceramtec Aktiengesellschaft Verfahren zum aufbauen strukturierter keramischer grünkörper
DE4235333C1 (de) * 1992-10-20 1994-03-03 Stoll Volker Verfahren zur Erzeugung von gerasterten Abbildungen auf Oberflächen
KR0127666B1 (ko) * 1992-11-25 1997-12-30 모리시다 요이찌 세라믹전자부품 및 그 제조방법
DE19643148C2 (de) * 1996-10-18 2003-08-28 Epcos Ag Herstellverfahren für keramische Körper mit Mikrostruktur und Verwendungen
DE19709691A1 (de) * 1997-03-10 1998-09-17 Siemens Ag Verfahren zur Herstellung eines strukturierten keramischen Körpers mit zumindest teilweise separierten Teilstrukturen
DE10037818A1 (de) * 2000-08-03 2002-03-07 Bosch Gmbh Robert Verfahren zur Strukturierung ungebrannter Schichten
US20100071614A1 (en) * 2008-09-22 2010-03-25 Momentive Performance Materials, Inc. Fluid distribution apparatus and method of forming the same
WO2015137248A1 (ja) * 2014-03-14 2015-09-17 Jsr株式会社 配線の製造方法、感放射線性組成物、電子回路および電子デバイス
CN104681274A (zh) * 2015-02-04 2015-06-03 深圳顺络电子股份有限公司 一种片式电子元器件内电极的制备方法
JP6608595B2 (ja) * 2015-02-17 2019-11-20 日本特殊陶業株式会社 トンネル付きセラミック部材の製造方法

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EP1145123A2 (de) * 1999-02-23 2001-10-17 Microchip Technology Inc. Kalibrierungsfunktionen von einer integrierten schaltung und speicherung von kalibrierungsparametern hierfür in einem programmierbaren sicherungsfeld

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Publication number Priority date Publication date Assignee Title
FR919911A (fr) * 1946-01-09 1947-03-21 Procédé pour l'obtention de motifs en relief dans de la poterie et poterie munie de motifs en relief suivant ce procédé
DE2142535A1 (de) * 1970-08-25 1972-03-02 Ibm Verfahren zum Herstellen von elektri sehen Mehrlagen Schaltungen auf kerami scher Basis
US3703864A (en) * 1970-11-02 1972-11-28 Magnacheck Corp Micr imprinting photo-etched credit card
FR2455499A1 (fr) * 1979-04-11 1980-11-28 Bing & Grondahl Porcelainfab Procede pour fabriquer un article en ceramique comportant un dessin ajoure
US4528260A (en) * 1983-04-27 1985-07-09 Rca Corporation Method of fabricating lenticular arrays
US4876179A (en) * 1986-06-13 1989-10-24 Siemens Aktiengesellschaft Method for manufacturing ceramic material having piezo-electric properties
EP1145123A2 (de) * 1999-02-23 2001-10-17 Microchip Technology Inc. Kalibrierungsfunktionen von einer integrierten schaltung und speicherung von kalibrierungsparametern hierfür in einem programmierbaren sicherungsfeld

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1174766A2 (de) * 2000-07-12 2002-01-23 E.I. Du Pont De Nemours And Company Verfahren zur Strukturierung einer nicht-bilderzeugenden keramischen Schicht
US6653056B2 (en) 2000-07-12 2003-11-25 E. I. Du Pont Nemours And Company Process for patterning non-photoimagable ceramic tape
EP1174766A3 (de) * 2000-07-12 2004-01-28 E.I. Du Pont De Nemours And Company Verfahren zur Strukturierung einer nicht-bilderzeugenden keramischen Schicht
US20130022809A1 (en) * 2011-07-18 2013-01-24 Technische Universitaet Wien Multilayer Ceramic Structure and Method for Producing the Same
US8840797B2 (en) * 2011-07-18 2014-09-23 Micro Systems Engineering Gmbh Multilayer ceramic structure and method for producing the same

Also Published As

Publication number Publication date
JPH02500427A (ja) 1990-02-15
JPH0530602B2 (de) 1993-05-10
WO1988008360A1 (en) 1988-11-03
DE3864264D1 (de) 1991-09-19
DE3713987A1 (de) 1988-11-10
EP0362213B1 (de) 1991-08-14
EP0362213A1 (de) 1990-04-11

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